顶空固相微萃取-气相色谱-质谱法测定皮革中的富马酸二甲酯

Determination of Dimethyl Fumarate in Leathers by Headspace Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

为了检测皮革中的富马酸二甲酯,采用顶空固相微萃取(HS-SPME)气相色谱-质谱法(GC-MS),考察了萃取纤维涂层、平衡温度、平衡时间、萃取时间、解吸温度和时间对萃取效率的影响,确定最优的顶空条件,并评估该方法的性能。结果表明:最优的顶空条件为100μm PDMS萃取纤维涂层,平衡温度80℃,平衡时间15 min,萃取时间4 min,解吸温度260℃,解吸时间1 min。该方法在0.05~10 mg/kg范围内观察到良好的线性,相关系数(R^(2))高于0.998,检出限为0.023 mg/L,方法加标回收率范围为99.48%~102.67%。该方法可以满足皮革及其制品中的富马酸二甲酯日常检测需要。

In order to detect dimethyl fumarate in leathers,headspace solid-phase microextraction(HS-SPME)-gas chromatography-mass spectrometry(GC-MS)was utilized.The effects of extraction fiber coating,equilibrium temperature,equilibrium time,extraction time,desorption temperature and time on the extraction efficiency were studied,the optimal headspace conditions were determined,and the performance of the method was evaluated.The optimum conditions were obtained as below:the fiber coating extraction at 100μm PDMS,equilibrium temperature 80°C,equilibrium time 15 min,extraction time 4 min,desorption temperature 260°C and desorption time 1 min.This method showed a good linearity in the range of 0.05-10 mg/kg with a correlation coefficient(R^(2))of above 0.998.The limit of detection was 0.023 mg/L.The recycling rate of this method was in the range of 99.48%—106.27%.It can meet the daily analysis of dimethyl fumarate in leathers and its products.